IP Library Granted Patent US 9,418,779
Granted Patent B2
US 9,418,779 · App. 14/059,773 · Granted Aug 16, 2016

Process for preparing scalable quantities of high purity manganese bismuth magnetic materials for fabrication of permanent magnets

Inventors: Jung Pyung Choi (Richland, WA); Curt A. Lavender (Richland, WA); Guosheng Li (Richland, WA); Jun Cui (Richland, WA)
Assignee: BATTELLE MEMORIAL INSTITUTE
H01F1/047C22C1/02C22C1/04H01F1/08B22F2998/10B22F2999/00C22C2202/02
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Quick Facts
Patent No.
US 9,418,779
App. No.
14/059,773
Granted
Aug 16, 2016
Kind
B2
Abstract

A scalable process is detailed for forming bulk quantities of high-purity α-MnBi phase materials suitable for fabrication of MnBi based permanent magnets.

Claims (30)

1. A process for preparing a high-purity α-MnBi magnetic alloy, comprising:

melting manganese (Mn) metal and bismuth (Bi) metal together in a ratio that is greater in manganese (Mn) metal than in bismuth (Bi) metal to form an alloy comprising between about 40 wt % and about 50 wt % α-MnBi material and residual fractions of unreacted manganese (Mn) metal and unreacted bismuth (Bi) metal therein;

heat treating the alloy in an oxygen-free gas atmosphere at a first temperature less than or equal to about 266° C. for a time up to about 8 hours sufficient to form at least about 60 wt % α-MnBi material therein and a second temperature between about 266° C. and about 358° C. for a time up to about 5 hours sufficient to form a quantity of β-MnBi material therein;

cooling the alloy after heating at a rate between about 1° C. per minute to about 10° C. per minute to decompose the quantity of β-MnBi material therein to increase the quantity of α-MnBi material therein;

milling the alloy to agglomerate unreacted manganese (Mn) metal and unreacted bismuth (Bi) metal together therein and to fracture the α-MnBi material therefrom;

sieving the milled alloy to collect the fractured α-MnBi material as a powder comprised of particles thereof in a fraction separate from the agglomerated manganese (Mn) and bismuth (Bi) metals fraction; and

heat treating the fractured α-MnBi material fraction in a vacuum at a temperature selected between about 250° C. and about 300° C. for a time sufficient to form the high-purity α-MnBi magnetic alloy comprising at least about 90 wt % α-MnBi material therein.

2. The process of claim 1 , wherein the melting is performed in an arc melter or an induction melter.

3. The process of claim 1 , wherein the melting yields the alloy in the form of a solid pellet or solid ingot.

4. The process of claim 1 , wherein the milling is performed in a hand mill, a power mill, a roll mill, or an attrition mill.

5. The process of claim 1 , wherein the milling includes forming particles of α-MnBi material with an average size below about 45 microns (45 μm).

6. The process of claim 1 , wherein heat treating the fractured α-MnBi material fraction in vacuum includes removing residual (Bi) metal as a vapor from the fractured fraction at a vacuum pressure selected between about 1×10 −2 Torr and about 2×10 −5 Torr.

7. The process of claim 1 , wherein heat treating the fractured α-MnBi material fraction in vacuum includes reacting unreacted (Bi) metal and unreacted (Mn) metal therein to increase the quantity of α-MnBi material therein.

8. The process of claim 1 , wherein the steps of milling the alloy and heat treating the fractured α-MnBi material fraction in vacuum are performed iteratively to increase the quantity of α-MnBi material in the high-purity α-MnBi magnetic alloy to greater than about 95 wt %.

9. The process of claim 1 , wherein the steps of milling the alloy and heat treating the fractured α-MnBi material fraction in vacuum are performed iteratively to increase the quantity of α-MnBi material in the high-purity α-MnBi magnetic alloy to greater than about 90 wt % to about 99 wt %.

10. The process of claim 1 , wherein the high-purity α-MnBi magnetic alloy includes a mass greater than or equal to about 100 grams in a single process batch.

11. The process of claim 1 , wherein the high-purity α-MnBi magnetic alloy includes a mass greater than or equal to about 1 kilogram in a single process batch.

12. The process of claim 1 , further including magnetizing the high-purity α-MnBi magnetic alloy.

13. The process of claim 1 , wherein the high-purity α-MnBi magnetic alloy is incorporated as a component of a permanent magnet.

14. The process of claim 1 , wherein the high-purity α-MnBi alloy magnetic is incorporated as a component of a permanent magnet-containing device.

15. A process for preparing a high-purity α-MnBi magnetic alloy, comprising:

melting manganese (Mn) metal and bismuth (Bi) metal together in a selected ratio that is greater in manganese (Mn) metal than in bismuth (Bi) metal to form an alloy comprising between about 40 wt % and about 50 wt % α-MnBi material and residual fractions of unreacted manganese (Mn) metal and unreacted bismuth (Bi) metal therein;

heat treating the alloy in an oxygen-free atmosphere at a first temperature less than or equal to about 266° C. for a time sufficient to form at least about 60 wt % α-MnBi material therein and a second temperature between about 266° C. and about 358° C. for a time sufficient to form a quantity of β-MnBi material therein;

milling the alloy to agglomerate unreacted manganese (Mn) metal and unreacted bismuth (Bi) metal together therein and to fracture the at least about 60 wt % α-MnBi material therefrom into separate fractions; and

heat treating the fractured α-MnBi material fraction in a vacuum at a temperature selected between about 250° C. and about 300° C. for a time sufficient to form the high-purity α-MnBi magnetic alloy comprising at least about 90 wt % α-MnBi material therein.

16. The process of claim 15 , wherein the oxygen-free atmosphere includes a reducing gas.

17. The process of claim 15 , wherein heat treating the alloy includes a time at the first temperature up to about 8 hours, and a time at the second temperature up to about 5 hours, respectively.

18. The process of claim 15 , further including cooling the alloy after heat treating at the second temperature at a rate between about 1° C. per minute and about 10° C. per minute to decompose the quantity of β-MnBi material therein to increase the quantity of α-MnBi material formed therein.

19. The process of claim 15 , wherein milling the alloy includes sieving the alloy to collect the fractured α-MnBi material fraction as particles of a selected size.

20. The process of claim 15 , wherein heat treating the fractured α-MnBi material fraction in vacuum includes removing residual (Bi) metal as a vapor from the fractured fraction at a vacuum pressure selected between about 1×10 −2 Torr and about 2×10 −5 Torr.

Assignments (2)
CONFIRMATORY LICENSE Recorded Dec 16, 2013
From: BATTELLE MEMORIAL INSTITUTE, PACIFIC NORTHWEST DIVISION
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 031828/0831 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 14, 2013
From: CHOI, JUNG-PYUNG; LAVENDER, CURT A.; LI, GUOSHENG; CUI, JUN
To: BATTELLE MEMORIAL INSTITUTE
Reel/Frame 031606/0047 →
Continuity (1)
Related Publication 20150110664A1 · Apr 23, 2015